CN101318816A - Method for manufacturing bismuth lanthanum titanate (BLT) ferro-electricity film at low-temperature - Google Patents
Method for manufacturing bismuth lanthanum titanate (BLT) ferro-electricity film at low-temperature Download PDFInfo
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- CN101318816A CN101318816A CNA2008100629164A CN200810062916A CN101318816A CN 101318816 A CN101318816 A CN 101318816A CN A2008100629164 A CNA2008100629164 A CN A2008100629164A CN 200810062916 A CN200810062916 A CN 200810062916A CN 101318816 A CN101318816 A CN 101318816A
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Abstract
The invention relates to a method for preparing a BLT ferroelectric film used for a ferroelectric storage at a low temperature. The preparation method consists of the complexing agent technique and the hydro-thermal reaction low temperature preparation technique. Firstly, the complexing agent technique is adopted, a BLT precursor solution is prepared by taking inorganic salt as a raw material and a film with required thickness is coated on the cleaned Pt/Ti/SiO2Si underlay rotationally, the thermal treatment is performed at a temperature of between 350 and 450 DEG C, and then the film after the thermal treatment is put into a high pressure reaction kettle to perform the hydro-thermal chemical reaction; the reaction temperature is between 150 and 300 DEG C, the reaction time lasts for 2 to 48 hours; the product is cooled in the furnace, washed and dried at a temperature of 80 DEG C so that the BLT ferroelectric film with the thickness between 400 and 900 nanometers is produced. The method has simple preparation technology, low preparation temperature, convenient operation and low cost and can be compatible with the microelectronic technology.
Description
Technical field
The present invention relates to laminated perovskite type Bi
3.15La
0.75Ti
3O
12(BLT) preparation method of ferroelectric membranc, the low temperature preparation method that particularly adopts complexing agent complexing technology to combine with the hydro-thermal reaction technology.
Background technology
Along with ferroelectric RAM (FRAM) has obtained increasingly extensive application with table in the middle of (as ammeter, water meter, gas meter etc.), measurement and medical instrumentation, contact type intelligent card, gate control system and the automobile black box in various public utilities.FRAM is the main research and development direction of current ferroelectric film memory, is the field of attaching great importance in the world.As the FRAM material, two kinds of materials that are considered to have an opportunity most are Pb-based lanthanumdoped zirconate titanates (PZT) and strontium bismuth tantalate (SBT), and wherein PZT has preferable ferroelectric properties, preparation temperature lower (600 ℃), but it has the problem of polarization fatigue and Lead contamination.Strontium bismuth titanate (SBT) material is known as does not have fatigue, but the preparation temperature of SBT higher (750 ℃), remaining polarization value is less, and spontaneous polarization appears at the α direction of principal axis that film is difficult for taking place preferred orientation.FRAM becomes more meticulous and the needs of lower voltage in order to satisfy, people also developed such as bismuth lanthanum titanate (BLT-(and Bi, La)
4Ti
3O
12) wait the ferroelectric material of other kinds.BLT will be as the ferroelectric material of next breakthrough development, because it has the ratio of remaining polarization value and saturated polarization value near 1.The various means of the preparation of BLT ferroelectric thin-flim materials, the method layer goes out constantly.Mainly contain the physics method and comprise magnetron sputtering and pulsed laser deposition etc., this class methods raw material is easy to get, but the membrane equipment complex and expensive, multi-component material is wayward; Chemical method comprises vapor phase process and liquid phase method.Vapor phase process comprises chemical Vapor deposition process, metal-organic decomposition method and metallorganics forensic chemistry vapour deposition process etc.; Liquid phase method comprises sol-gel method, superpolymer precursor process etc.No matter be vapor phase process or liquid phase method, the raw material of use all is the metal organic salt compound, and is very expensive.And the ferroelectric membranc leakage current of Prepared by Sol Gel Method is bigger, and film-forming temperature is higher.How at standard type Pt/Ti/SiO
2Realize the laminated perovskite type on the/Si substrate: bismuth lanthanum titanate (BLT) ferroelectric membranc is a problem demanding prompt solution.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art.With the inorganics is raw material, adopts complexing agent complexing technology, utilizes the inorganic salt liquid chemical method low temperature that combines with hydro-thermal reaction to prepare bismuth lanthanum titanate (BLT) ferroelectric membranc.Preparation technology is simple for this method, and preparation temperature is low, easy to operate, and cost is lower, can with the microelectronics compatibility.
Technical scheme of the present invention is as follows:
One: the precursor solution preparation
Be Bi: La: Ti=3.15 * (1.00-1.06) in molar ratio: 0.75: 3 weighing Bismuth trinitrate (Bi (NO
3)
35H
2O), lanthanum nitrate (La (NO
3)
36H
2O), butyl (tetra) titanate (Ti (C
4H
9O)
4) wait three kinds of components, wherein * (1.00-1.06) be because the Bi component has certain volatilization in follow-up heat treatment process, with the excessive 0-10mol% of Bi component.Employing is with Bismuth trinitrate, lanthanum nitrate, and butyl (tetra) titanate, ethylene glycol and ammoniacal liquor etc. is starting material, is intercalating agent with the citric acid.
With a certain amount of Bismuth trinitrate and lanthanum nitrate and mixing, add the aqueous citric acid solution of equimolar amount by stoichiometric ratio, use the magnetic stirrer heating also to stir, keeping temperature is 45-55 ℃, dissolve fully up to this blended solid, obtain bismuth-containing, in the citric acid solution of lanthanum.The pH value that a certain amount of butyl (tetra) titanate is added to equimolar amount is in the citric acid solution of 6-7, and heated and stirred maintains the temperature at 50-70 ℃, form the stable faint yellow transparent solution that is, and and bismuth-containing, the citric acid solution of lanthanum mixes, and obtains containing the precursor solution of Ba, La and Ti; By viscosity, pH value (6-7) and the cumulative volume of spent glycol and ammoniacal liquor regulator solution, after fully stirring, filtration made 0.1-0.5mol/L and got flaxen precursor solution more than 3 hours the reaction times.
Two. on sol evenning machine, get rid of film.
Cleaned Pt/Ti/SiO on photoresist spinner
2On/Si the substrate, drip and go up a certain amount of precursor solution, with certain speed of rotation rotation, speed of rotation 2000-5000rps, the even glue time is 10-40 hour, directly deposits bismuth lanthanum titanate (BLT) ferroelectric membranc wet film;
Three. the heat treatment process of bismuth lanthanum titanate (BLT) ferroelectric membranc wet film
1) drying process: in the infrared microwave stove 100 ℃-150 ℃ dry 5-30 minute;
2) heat treatment process: put into quartz tube furnace, room temperature rises to 350 ℃-450 ℃ with 150 ℃/hour of temperature rise rates, oxygen flow be the 1-6 liter/minute mobile oxidizing atmosphere under thermolysis 10-50 minute; Furnace cooling repeats repeatedly above-mentioned whirl coating-heat treatment process, forms to have certain crystallization phases composition and uniform film;
Four. the preparation of bismuth lanthanum titanate (BLT) ferroelectric membranc low temperature
Bismuth lanthanum titanate (BLT) precursor solution that adds the step 1 preparation in the autoclave makes that contained species of metal ion adapts in the species of metal ion film in the hydrothermal solution, and adopts ammonia soln to regulate pH value 8-10, the compactedness control 75% of solution.To obtain having certain crystallization phases is formed and uniformly film put into autoclave and carry out hydrothermal chemical reaction.Temperature of reaction 150-300 ℃, reaction times 2-30 hour; Furnace cooling, the washing, 60-90 ℃ of oven dry, obtain bismuth lanthanum titanate (BLT) ferroelectric thin-flim materials of the thickness of 400-900nm.
Method provided by the invention is implemented convenient, and less demanding to experimental installation, cost is low; In order to improve film performance, adopt the glassy phase compounding technology, change the sticking power of film and substrate, reduce the leakage current of film; The ferroelectric membranc of the inventive method preparation has good electric property, can be used for storer and makes.
Specific embodiments
The invention will be further described below in conjunction with embodiment:
Embodiment 1:
One: the precursor solution preparation
Weighing Bismuth trinitrate (Bi (NO in molar ratio
3)
35H
2O) 0.03445mol, lanthanum nitrate (La (NO
3)
36H
2O) 0.0075mol, butyl (tetra) titanate (Ti (C
4H
9O)
4) three kinds of components of 0.03mol, citric acid 0.15mol.Load weighted Bismuth trinitrate and lanthanum nitrate are mixed, added the aqueous citric acid solution of respective amount in 1: 2 in molar ratio, use magnetic stirrer heating and stirring, keeping temperature is 45-55 ℃, dissolves fully up to this blended solid, obtains bismuth-containing, in the citric acid solution of lanthanum.It is that the corresponding mol ratio of 6-7 is in 1: 2 the citric acid solution that load weighted butyl (tetra) titanate is added to pH value, heated and stirred, maintain the temperature at 50-70 ℃, form the stable faint yellow transparent solution that is, and and bismuth-containing, the citric acid solution of lanthanum mixes, and obtains containing the precursor solution of Ba, La and Ti; By viscosity, pH value and the cumulative volume of spent glycol and ammoniacal liquor regulator solution, obtaining strength of solution is 0.1mol/L solution, after fully stirring, filters and makes flaxen precursor solution.
Two. whirl coating on sol evenning machine.
Cleaned Pt/Ti/SiO on photoresist spinner
2On/Si the substrate, drip and go up a certain amount of precursor solution, with certain speed of rotation rotation, speed of rotation 2000-5000rps, the even glue time is 10-40s, directly deposits bismuth lanthanum titanate (BLT) ferroelectric membranc wet film;
Three. the thermal treatment of bismuth lanthanum titanate (BLT) ferroelectric membranc wet film
1) drying process: 100 ℃ of-150 ℃ of dryings are 15 minutes in the infrared microwave stove;
2) heat treatment process: put into quartz tube furnace, room temperature rises to 400 ℃ with 150 ℃/hour of temperature rise rates, oxygen flow be the 1-6 liter/minute mobile oxidizing atmosphere under thermolysis 30 minutes; Furnace cooling repeats 4 times above-mentioned whirl coating-heat treatment process, forms to have certain crystallization phases composition and uniform film;
Four. the preparation of bismuth lanthanum titanate (BLT) ferroelectric membranc low temperature
Bismuth lanthanum titanate (BLT) precursor solution that adds the preparation of embodiment 1 step 1 in the autoclave, make that contained species of metal ion adapts in the species of metal ion film in the hydrothermal solution, and adopt ammonia soln to regulate pH value 8, the compactedness control 75% of solution.To obtain having certain crystallization phases is formed and uniformly film put into autoclave and carry out hydrothermal chemical reaction.200 ℃ of temperature of reaction, 10 hours reaction times; Furnace cooling, the washing, 60 ℃ of oven dry, obtain bismuth lanthanum titanate (BLT) ferroelectric thin-flim materials of the thickness of 500nm-600nm.
Embodiment 2:
One: the precursor solution preparation
Weighing Bismuth trinitrate (Bi (NO in molar ratio
3)
35H
2O) 0.03445mol, lanthanum nitrate (La (NO
3)
36H
2O) 0.0075mol, butyl (tetra) titanate (Ti (C
4H
9O)
4) three kinds of components such as 0.03mol, citric acid 0.15mol.Load weighted Bismuth trinitrate and lanthanum nitrate are mixed, added the aqueous citric acid solution of respective amount in 1: 2 in molar ratio, use magnetic stirrer heating and stirring, keeping temperature is 45-55 ℃, dissolves fully up to this blended solid, obtains bismuth-containing, in the citric acid solution of lanthanum.It is that the corresponding mol ratio of 6-7 is that heated and stirred maintains the temperature at 50-70 ℃ in 1: 2 the citric acid solution that load weighted butyl (tetra) titanate is added to pH value, form the stable faint yellow transparent solution that is, and and bismuth-containing, the citric acid solution of lanthanum mixes, and obtains containing the solution of Ba, La and Ti; The cumulative volume of viscosity, pH value and colloidal sol by spent glycol and ammoniacal liquor regulator solution, obtaining strength of solution is 0.1mol/L solution, after fully stirring, filters and makes flaxen precursor solution.
Two. on sol evenning machine, get rid of film.
Cleaned Pt/Ti/SiO on photoresist spinner
2On/Si the substrate, drip and go up certain quantity solution, with certain speed of rotation rotation, speed of rotation 2000-5000rps, the even glue time is 10-40 hour, directly deposits bismuth lanthanum titanate (BLT) ferroelectric membranc wet film;
Three. the thermal treatment of bismuth lanthanum titanate (BLT) ferroelectric membranc wet film
1) drying process: 100 ℃ of-150 ℃ of dryings are 15 minutes in the infrared microwave stove;
2) heat treatment process: put into quartz tube furnace, room temperature rises to 400 ℃ with 150 ℃/hour of temperature rise rates, oxygen flow be the 1-6 liter/minute mobile oxidizing atmosphere under thermolysis 30 minutes; Furnace cooling repeats 4 times above-mentioned whirl coating-heat treatment process, forms to have certain crystallization phases composition and uniform film;
Four. the preparation of bismuth lanthanum titanate (BLT) ferroelectric membranc low temperature
Bismuth lanthanum titanate (BLT) precursor solution that adds the preparation of embodiment 2 step 1 in the autoclave, make that contained species of metal ion adapts in the species of metal ion film in the hydrothermal solution, and adopt ammonia soln to regulate pH value 8.5, the compactedness control 75% of solution.To obtain having certain crystallization phases is formed and uniformly film put into autoclave and carry out hydrothermal chemical reaction.240 ℃ of temperature of reaction, 12 hours reaction times; Furnace cooling, the washing, 80 ℃ of oven dry, obtain bismuth lanthanum titanate (BLT) ferroelectric thin-flim materials of the thickness of 600nm-700nm.
Embodiment 3:
One: the precursor solution preparation
Weighing Bismuth trinitrate (Bi (NO in molar ratio
3)
35H
2O) 0.03445mol, lanthanum nitrate (La (NO
3)
36H
2O) 0.0075mol, butyl (tetra) titanate (Ti (C
4H
9O)
4) three kinds of components of 0.03mol, citric acid 0.15mol.Load weighted Bismuth trinitrate and lanthanum nitrate are mixed, added the aqueous citric acid solution of respective amount in 1: 2 in molar ratio, use magnetic stirrer heating and stirring, keeping temperature is 45-55 ℃, dissolves fully up to this blended solid, obtains bismuth-containing, in the citric acid solution of lanthanum.It is that the corresponding mol ratio of 6-8 is that heated and stirred maintains the temperature at 50-70 ℃ in 1: 2 the citric acid solution that load weighted butyl (tetra) titanate is added to pH value, form the stable faint yellow transparent solution that is, and and bismuth-containing, the citric acid solution of lanthanum mixes, and obtains containing the solution of Ba, La and Ti; By viscosity, pH value and the cumulative volume of spent glycol and ammoniacal liquor regulator solution, obtaining strength of solution is 0.2mol/L solution, after fully stirring, filters and makes flaxen precursor solution.
Two. on sol evenning machine, get rid of film.
Cleaned Pt/Ti/SiO on photoresist spinner
2On/Si the substrate, drip and go up a certain amount of precursor solution, with certain speed of rotation rotation, speed of rotation 2000-5000rps, the even glue time is 10-40s, directly deposits bismuth lanthanum titanate (BLT) ferroelectric membranc wet film;
Three. the thermal treatment of bismuth lanthanum titanate (BLT) ferroelectric membranc wet film
1) drying process: 100 ℃ of-150 ℃ of dryings are 15 minutes in the infrared microwave stove;
2) heat treatment process: put into quartz tube furnace, room temperature rises to 450 ℃ with 150 ℃/hour of temperature rise rates, oxygen flow be the 1-6 liter/minute mobile oxidizing atmosphere under thermolysis 30 minutes; Furnace cooling repeats 4 times above-mentioned whirl coating-heat treatment process, forms to have certain crystallization phases composition and uniform film;
Four. the preparation of bismuth lanthanum titanate (BLT) ferroelectric membranc low temperature
Bismuth lanthanum titanate (BLT) precursor solution that adds the preparation of embodiment 2 step 1 in the autoclave, make that contained species of metal ion adapts in the species of metal ion film in the hydrothermal solution, and adopt ammonia soln to regulate pH value 9, the compactedness control 75% of solution.To obtain having certain crystallization phases is formed and uniformly film put into autoclave and carry out hydrothermal chemical reaction.270 ℃ of temperature of reaction, 15 hours reaction times; Furnace cooling, the washing, 90 ℃ of oven dry, obtain bismuth lanthanum titanate (BLT) ferroelectric thin-flim materials of the thickness of 700nm-800nm.
Embodiment 4:
One: the precursor solution preparation
Weighing Bismuth trinitrate (Bi (NO in molar ratio
3)
35H
2O) 0.03445mol, lanthanum nitrate (La (NO
3)
36H
2O) 0.0075mol, butyl (tetra) titanate (Ti (C
4H
9O)
4) three kinds of components such as 0.03mol, citric acid 0.15mol.Load weighted Bismuth trinitrate and lanthanum nitrate are mixed, added the aqueous citric acid solution of respective amount in 1: 2 in molar ratio, use magnetic stirrer heating and stirring, keeping temperature is 45-55 ℃, dissolves fully up to this blended solid, obtains bismuth-containing, in the citric acid solution of lanthanum.It is that the corresponding mol ratio of 6-8 is that heated and stirred maintains the temperature at 50-70 ℃ in 1: 2 the citric acid solution that load weighted butyl (tetra) titanate is added to pH value, form the stable faint yellow transparent solution that is, and and bismuth-containing, the citric acid solution of lanthanum mixes, and obtains containing the solution of Ba, La and Ti; By viscosity, pH value and the cumulative volume of spent glycol and ammoniacal liquor regulator solution, obtaining strength of solution is 0.2mol/L solution, after fully stirring, filters and makes flaxen precursor solution.
Two. on sol evenning machine, get rid of film.
Cleaned Pt/Ti/SiO on photoresist spinner
2On/Si the substrate, drip and go up a certain amount of precursor solution, with certain speed of rotation rotation, speed of rotation 2000-5000rps, the even glue time is 10-40 hour, directly deposits bismuth lanthanum titanate (BLT) ferroelectric membranc wet film;
Three. the thermal treatment of bismuth lanthanum titanate (BLT) ferroelectric membranc wet film
1) drying process: 100 ℃ of-150 ℃ of dryings are 15 minutes in the infrared microwave stove;
2) heat treatment process: put into quartz tube furnace, room temperature rises to 400 ℃ with 150 ℃/hour of temperature rise rates, oxygen flow be the 1-6 liter/minute mobile oxidizing atmosphere under thermolysis 30 minutes; Furnace cooling repeats 6 times above-mentioned whirl coating-heat treatment process, forms to have certain crystallization phases composition and uniform film;
Four. the preparation of bismuth lanthanum titanate (BLT) ferroelectric membranc low temperature
Bismuth lanthanum titanate (BLT) precursor solution that adds the preparation of embodiment 4 step 1 in the autoclave, make that contained species of metal ion adapts in the species of metal ion film in the hydrothermal solution, and adopt ammonia soln to regulate pH value 10, the compactedness control 75% of solution.To obtain having certain crystallization phases is formed and uniformly film put into autoclave and carry out hydrothermal chemical reaction.300 ℃ of temperature of reaction, 10 hours reaction times; Furnace cooling, the washing, 70 ℃ of oven dry, obtain bismuth lanthanum titanate (BLT) ferroelectric thin-flim materials of the thickness of 800-900nm.
At last, should be pointed out that above embodiment only is the more representational example of the present invention.Obviously, technical scheme of the present invention is not limited to the foregoing description, and many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (3)
1, bismuth lanthanum titanate Bi
3.15La
0.75Ti
3O
12(BLT) precursor solution, it is characterized in that: adopting with Bismuth trinitrate, lanthanum nitrate, butyl (tetra) titanate, ethylene glycol and ammoniacal liquor etc. is starting material, with the citric acid is intercalating agent, ferroelectric phase component: Bismuth trinitrate, lanthanum nitrate, the mol ratio of butyl (tetra) titanate are Bi: La: Ti=3.15 * (1.00-1.10): 0.75: 3.
2, according to bismuth lanthanum titanate (BLT) the precursor solution preparation method of claim 1, it is characterized in that: a certain amount of Bismuth trinitrate and lanthanum nitrate are also mixed by stoichiometric ratio, add a certain amount of aqueous citric acid solution, use magnetic stirrer heating and stirring, keeping temperature is 45-55 ℃, dissolve fully up to this blended solid, obtain bismuth-containing, in the citric acid solution of lanthanum; A certain amount of butyl (tetra) titanate is added in a certain amount of citric acid solution that pH value is 6-7, and heated and stirred maintains the temperature at 50-70 ℃, form the stable faint yellow transparent solution that is, and and bismuth-containing, the citric acid solution of lanthanum mixes, and obtains containing the precursor solution of Ba, La and Ti; By the viscosity and the pH value of spent glycol and ammoniacal liquor regulator solution, after fully stirring, filtration made 0.1-0.5mol/L and got flaxen precursor solution more than 3 hours the reaction times.
3, bismuth lanthanum titanate (BLT) ferroelectric membranc preparation method is characterized in that:
One. the preparation of bismuth lanthanum titanate (BLT) precursor solution:
With a certain amount of Bismuth trinitrate and lanthanum nitrate and mixing, add a certain amount of aqueous citric acid solution by stoichiometric ratio, use the magnetic stirrer heating also to stir, keeping temperature is 45-55 ℃, dissolves fully up to this blended solid, obtains bismuth-containing, in the citric acid solution of lanthanum; A certain amount of butyl (tetra) titanate is added in a certain amount of citric acid solution that pH value is 6-7, and heated and stirred maintains the temperature at 50-70 ℃, form the stable faint yellow transparent solution that is, and and bismuth-containing, the citric acid solution of lanthanum mixes, and obtains containing the precursor solution of Ba, La and Ti; By viscosity, pH value and the cumulative volume of spent glycol and ammoniacal liquor regulator solution, after fully stirring, filtration made 0.1-0.5mol/L and got flaxen bismuth lanthanum titanate (BLT) precursor solution more than 3 hours the reaction times;
Two. on sol evenning machine, get rid of film
Cleaned Pt/Ti/SiO on photoresist spinner
2On/Si the substrate, drip and go up a certain amount of precursor solution, with certain speed of rotation rotation, speed of rotation 2000-5000rps, the even glue time is 10-40 hour, directly deposits bismuth lanthanum titanate (BLT) ferroelectric membranc wet film;
Three.: the thermal treatment of bismuth lanthanum titanate (BLT) ferroelectric membranc wet film
1) drying process: in the infrared microwave stove 100 ℃-150 ℃ dry 5-30 minute;
2) heat treatment process: put into quartz tube furnace, room temperature rises to 350 ℃-450 ℃ with 150 ℃/hour of temperature rise rates, oxygen flow be the 1-6 liter/minute mobile oxidizing atmosphere under thermolysis 10-50 minute; Furnace cooling repeats repeatedly above-mentioned whirl coating-heat treatment process, forms to have certain crystallization phases composition and uniform film;
Four. the preparation of bismuth lanthanum titanate (BLT) ferroelectric membranc low temperature
Bismuth lanthanum titanate (BLT) precursor solution that adds the step 1 preparation in the autoclave, make that contained species of metal ion adapts in the species of metal ion film in the hydrothermal solution, and adopt ammonia soln to regulate pH value 8-10, the compactedness control 75% of solution, to obtain having certain crystallization phases is formed and uniformly film put into autoclave and carry out hydrothermal chemical reaction, temperature of reaction 150-300 ℃, reaction times 2-30 hour; Furnace cooling, the washing, 60-90 ℃ of oven dry, obtain bismuth lanthanum titanate (BLT) ferroelectric thin-flim materials of the thickness of 400-900nm.
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| CN101811889A (en) * | 2010-04-27 | 2010-08-25 | 济南大学 | Lanthanide-doped bismuth titanate film and preparation method thereof |
| CN104538176A (en) * | 2014-12-05 | 2015-04-22 | 黑龙江省科学院高技术研究院 | Method for crystallizing bismuth titanate ferroelectric film by high pressure |
| CN106810238A (en) * | 2017-01-20 | 2017-06-09 | 武汉理工大学 | A kind of rear-earth-doped different-shape bismuth titanates nano-crystal film and preparation method thereof |
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| CN111003944A (en) * | 2019-12-16 | 2020-04-14 | 新昌中国计量大学企业创新研究院有限公司 | Rare earth ion Eu3+Doping with Bi3LaTi3O12Ferroelectric glass-ceramic up-conversion luminescent powder |
| CN114907117A (en) * | 2022-04-21 | 2022-08-16 | 清华大学 | Bismuth titanate-based ceramic material and preparation method and application thereof |
| CN116283276A (en) * | 2023-04-07 | 2023-06-23 | 广西华锡集团股份有限公司 | La-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof |
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| CN101811889B (en) * | 2010-04-27 | 2012-07-25 | 济南大学 | Lanthanide-doped bismuth titanate film and preparation method thereof |
| CN101811889A (en) * | 2010-04-27 | 2010-08-25 | 济南大学 | Lanthanide-doped bismuth titanate film and preparation method thereof |
| CN104538176A (en) * | 2014-12-05 | 2015-04-22 | 黑龙江省科学院高技术研究院 | Method for crystallizing bismuth titanate ferroelectric film by high pressure |
| CN108883035B (en) * | 2016-04-06 | 2021-09-28 | 兰达拉伯斯（2012）有限公司 | UV-protective composition and use thereof |
| CN108883035A (en) * | 2016-04-06 | 2018-11-23 | 兰达拉伯斯（2012）有限公司 | UV protection component and application thereof |
| CN106810238A (en) * | 2017-01-20 | 2017-06-09 | 武汉理工大学 | A kind of rear-earth-doped different-shape bismuth titanates nano-crystal film and preparation method thereof |
| CN111003944A (en) * | 2019-12-16 | 2020-04-14 | 新昌中国计量大学企业创新研究院有限公司 | Rare earth ion Eu3+Doping with Bi3LaTi3O12Ferroelectric glass-ceramic up-conversion luminescent powder |
| CN114907117A (en) * | 2022-04-21 | 2022-08-16 | 清华大学 | Bismuth titanate-based ceramic material and preparation method and application thereof |
| CN114907117B (en) * | 2022-04-21 | 2023-04-21 | 清华大学 | Bismuth titanate-based ceramic material and preparation method and application thereof |
| CN116283276A (en) * | 2023-04-07 | 2023-06-23 | 广西华锡集团股份有限公司 | La-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof |
| CN116332641A (en) * | 2023-04-07 | 2023-06-27 | 广西华锡集团股份有限公司 | Yb-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof |
| CN116283276B (en) * | 2023-04-07 | 2024-02-06 | 广西华锡集团股份有限公司 | La-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof |
| CN116332641B (en) * | 2023-04-07 | 2024-04-12 | 广西华锡集团股份有限公司 | Yb-Sn co-doped bismuth titanate-based ferroelectric film and preparation method thereof |
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